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溶剂解吸-气相色谱法测定工作场所空气中二乙烯三胺

[Determination of diethylenetriamine in workplace air by solvent desorption-gas chromatography].

作者信息

Feng Di, Du Hao, Yan Meng

机构信息

Occupational Hygiene Technology Services Co. , Ltd. NHWOC, Zhanjiang 524057, China.

出版信息

Wei Sheng Yan Jiu. 2020 Jan;49(1):118-122. doi: 10.19813/j.cnki.weishengyanjiu.2020.01.021.

Abstract

OBJECTIVE

To establish solvent desorption gas chromatograph method for diethylenetriamine determination in workplace air.

METHODS

Diethylenetriamine in workplace air was collected with alkaline silicone tube, and desorbed with 0. 2 mol/L methanol solution of hydrochloric acid. After centrifugation, the supernatant neutralized with 0. 3 mol/L methanol solution of potassium hydroxide, was separated with 5%-phenyl-methyl polysiloxane(HP-5)(25 m×0. 32 mm×0. 52 mm)and measured with flame ionization detector.

RESULTS

Detection limit of the method was 0. 49 μg/mL, quantification limit of the method was 1. 64 μg/mL, quantitative determination range of method was 1. 64-233. 80 μg/mL, and the minimum quantitative determination concentration was 0. 22 mg/m~3(based on 7. 5 L sample). The method had a good reproducibility, the relative standard deviation was 1. 4%-3. 3%, the average of desorption efficiency was 90. 8%, and the average of sampling efficiency was 93. 2%. The penetrating capacity of 200 mg alkaline silicone was over than 7. 1 mg, and the samples at room temperature could be preserved for 15 days at least. Ethylenediamine, triethylenetetramine or tetraethylenepentamine coexisted in the air did not interfere during the determination of diethylenetriamine.

CONCLUSION

The method with low determination concentration, high accuracy and precision, is feasible for determination of diethylenetriamine in workplace air.

摘要

目的

建立工作场所空气中二乙烯三胺的溶剂解吸气相色谱测定方法。

方法

用碱性硅胶管采集工作场所空气中的二乙烯三胺,用0.2mol/L盐酸甲醇溶液解吸。离心后,用0.3mol/L氢氧化钾甲醇溶液中和上清液,用5%-苯基-甲基聚硅氧烷(HP-5)(25m×0.32mm×0.52mm)分离,用火焰离子化检测器测定。

结果

该方法的检出限为0.49μg/mL,定量限为1.64μg/mL,定量测定范围为1.64 - 233.80μg/mL,最低定量测定浓度为0.22mg/m³(以7.5L样品计)。该方法具有良好的重现性,相对标准偏差为1.4% - 3.3%,解吸效率平均为90.8%,采样效率平均为93.2%。200mg碱性硅胶的穿透容量超过7.1mg,室温下样品至少可保存15天。空气中共存的乙二胺、三乙烯四胺或四乙烯五胺在二乙烯三胺测定过程中不产生干扰。

结论

该方法测定浓度低、准确度和精密度高,可用于工作场所空气中二乙烯三胺的测定。

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